Sulfo-fatty-aromatic acid salt.



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nnustr 'iWITCI-IELL, or WYOMING, 01-110;

SULFO-FATTY AROMA'1IC ACID SALT.

No Drawing.

To all whom it may concern:

Be it known that LEnnsT TWITGHELL, a citizen of the United States,residing at \Vyom'ing, in the county of Hamilton and State of Ohio, haveinvented certain new and useful Improvements in Sulfo-Fatty- AromaticAcid Salt, of which the following is a specification.

My invention relates to a new product comprising a salt of a saponifying(hydrolyz erate an active, stable, pure and concentrated, sulfonic acidsaponifier, of an oily nature, and which will not decompose at thetemperature of boiling water under which the process is carried on, andthe metal component of the reagent uniting with the acid to form aproduct capable of beingseparated from the glycerin as a precipitate.This sulfonic material, being a stable powder or solid, can be safelyshipped in ordinary packages and does not requirethe use of sealedvessels, as when the conventional liquid saponifier is used. The drysolid sulfonic material can be more efficiently administered in thetreatment than a liquid saponifier, and can be used'in smallerquantities. But of still greater importance is the fact that thesulfonic acid when so liberated from the combination existing as-a drysolid or powder in the presence of the boiling fats or oils, becomes aconcentrated, pure and stable saponifier, far more intense in itssaponifying action than any liquid material adapted and used for thesame purpose. More specifically, it is the object of my invention torefine and concentrate the crude product known generically assulfo-fattyaromatic acid. such a product and a process of producing itbeing described and claimed in my prior Patent No. 682,503, dated July11, 1899.

A specific example ofthis ,saponifving reagent may be designated asnaphthalenestearo-sulfonic acid, and this example will Specification ofLetters Patent.

Patented Feb. 1, rate.

Application filed January 29, 1913. Serial No. 744,820.

serve to illustrate the principles on which my present invention isbased, the conversion of said product into a salt constituting one ofthe concrete embodiments of the series of products which it is theobject of this invention to produce. Under manufacturing conditionsobtaining, this product when produced in accordance with-the processdescribed in my said prior patent, exists as about a forty per cent.component of aviscous, dark-colored liquid, containing as impuritiesapproximately about thirty-five per cent. of oleic acid, which has beenacted upon, polymerized and colored by the sulfuric acid, andapproximately twenty-five per cent. of water containing some sulfuricacid and naphthalene-sulfonic acid. This crude product is an oily ortarry liquid almost black, and while it is and has been for many yearsadvantageously employed in the manufacture of fatty acids and glycerin,it is open to the objection that the active saponifying acid exists in anonrefined and non-concentrated condition.

"Also the oil slightly colors the fatty acid in the ultimate'saponifving process, while the naphthalene-sulfonic acid somewhatcontaminates the glycerin. Furthermore, inasmuch as this crude productexists as a heavy liquid, it requires shipping in sealed vessels thebulk of the product being considerable in proportion to the Weight ofthe active saponifying acid component.

It is the object of my present invention to refine and concentrate thiscrude product and convert it into a water-insoluble salt of thenaphthalene-stearo-sulfonic acid,

which can be separated, dried and powdered and shipped in condensedform. The'preferred process of treating this crude product'constitutesthe subject-matter ofa sep- ,arate application for Letters Patent, filedJanuary 29, 1913, Serial No. 744,818. It will sufiice for the presentpurpose to briefly recite the steps of this process as it is pref--erably employed.

The crude product of the naphthalenestearosulfonic acid is first treatedwith a solution of common salt in orderto Wash out the greater part ofthesulfuric acid' and aromatic sulfonic acid which it contains asimpurities. This treatment also converts part of'thesulfo-fatty-aromatic acid into its sodium salt (Water alone would not dofor this washing as the reagent is soluble in 'pure water, but insolublein water containing salt). Second, the material is put into a suitableextraction apparatus and extracted with naphtha or other solvent whichdissolves fats and fatty acids but not the sulfofatty-aromatic acid.This operation removes the free fatty matter which had been acted on andcolored by the sulfuric acid in the manufacture of the original reagentbut had not been converted into sulfo-fatty-aromatic acid. Operationsone and two may be advantageously combined into one. Third, theextracted material is dissolved in a large quantity of water andprecipitated with a salt of such a metal as will form an insolublecompound with the fatty-aromatic-sulfonic. acidsuch metals are barium,calcium, aluminum, magnesium, etc. As the sulfofatty-aromatic acid hasnot been completely neutralized with the salt water treatment, it may benecessary at this stage to add a small quantity of a base to neutralizethe mixture and cause. complete precipitation. It is to be understood,however, that the neutraliz- 'ing step need only be suliicient toneutralize the sulfonic component of the crude product, as the fattyacid component, being a relatively weak acid, need not be completelyneutralized. The remainder of the soluble impurities have been washedout by the process. Fourth, the precipitate, which sinks to the bottomof the tank as a viscous mass, is removed, dried and ground to powder.

The powder is stable and the major portion comprises a concentratedsaponifying agent. To test the strength of this product it is onlynecessary to determine the percentage of the sulfonic component thereof(radical, S0 11) as this constitutes the active saponifying principle ofthe material.

The residue of my new product, amounting to approximately fifteen ortwenty per cent, consists of oil or a little water, but without anyappreciable deleterious characteristics.

I thus obtain a solid which can be powdered as distinguished from theliquid product. The powder is nonhygroscopic, can be cheaply packed forshipping without danger of loss through leakage, and it is extremelystable.

I thus obtain a condensed, concentrated and stable sulfonic material,existing as a commercial dry solid or powder, the active, sulfonicsaponifier of which is relatively double strength as compared to theoriginal or crude product, and it can be administered as a powder orbroken up solid in the treatment process, in connection with asuflicient amount of mineral acid, such as sulfuricor hydrochloric acid,to react upon the material and liberate the active, stable sulfonic acidsaponifier, the metal component of the material forming a combinationwith the mineral acid which can be separated out as a precipitate.nitely, shipped conveniently in reduced bulk as a dry solid, and usedconveniently and economically when required, the saponifier efficiencyis increased, and a better product produced. This powdered form ofreagent is of a dull-grayish color, as a considerable amount of thedark-colored oil has been eliminated, so that lighter products resultfrom the use of this new reagent, and as all of the naphthalene-sulfonicacid has been removed, the glycerin produced as a result of the use ofmy present reagent is much purer than that obtained'by using the crudereagent.

Having described my invention, 1 claim A sulfonic material for themanufacture of glycerin and fatty acids from fats and oils, consistingof a dry, stable solid, insoluble in Water, consisting of a neutral bodyhaving the property when treated with a mineral acid of yielding anactive, concentrated sulfonic saponifier, of an oily nature, which willnot decompose at the temperature of boiling water, and a residue ofinnocuous character adapted to be removed as a precipitate.

\ In testimony whereof, I have hereunto set my hand.

ERNST TWITCHELL.

Witnesses OLIVER B. :KAISER, LOUISE A. BECK.

This material can be stored indefi

